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Continuous preparation method of tetraphenyl divalent monometal porphyrin

A tetraphenyl divalent mono-metalloporphyrin technology, applied in the direction of organic chemistry, etc., can solve the problems such as the large safety hazard of the mechanical stirring paddle of the equipment, the inability to judge whether the sedimentation tank is full, and the continuous inflow and outflow of materials is not realized, so as to avoid Oxidation intermittent operation risk, easy to expand production, avoid the effect of local hot spots

Inactive Publication Date: 2016-06-08
山东有言环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is essentially adding the solvent required for the reaction in batches, and then continuously adding the reactant tetraphenylporphine and metal salt into the stirred tank for reaction, which is no different from the batch operation of dropping operation, and is still a batch operation in essence. The process does not realize the continuous entry and exit of materials
And in the actual operation process, due to the characteristics of the system itself, the color of the reaction solution is completely opaque, and it is impossible to judge whether the settling tank is filled with TPPM in actual production. II
[0017] (2) The height-to-diameter ratio of the stirred reactor used in this method is 20-40:1, and the safety hazards of the equipment and machinery, especially the stirring paddle, are relatively large.
[0019] (4) The method does not realize that the continuous operation process will lead to the formation of explosive gas containing the solvent in the system, and there is a huge operational safety risk in the system, especially when the system contains the benzene, toluene, Xylene, dichloromethane, chloroform and other solvents are more likely to form explosive gases
The great danger and safety of introducing air into the above-mentioned several solvents did not mention any countermeasures

Method used

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  • Continuous preparation method of tetraphenyl divalent monometal porphyrin
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  • Continuous preparation method of tetraphenyl divalent monometal porphyrin

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Effect test

Embodiment 1

[0053] R in the general formula (I) tetraphenylporphin used 1 = H, R 2 = H, R 3 =H. Metal salt is MnCl 2 , the molar concentration is 0.15mol / L, and the solvent is a mixture of 90% by mass of DMF and 10% by mass of acetic acid. The molar concentration of tetraphenylporphine is 0.02mol / L, and the solvent is DMF. The volume flow rate of tetraphenylporphine solution is 0.64ml / L, and the molar flow ratio of metal salt to tetraphenylporphine is 3.7:1. The reaction pressure of the reactor is 0.2MPa, the reaction temperature is 146.1°C, and the residence time is 540s. Final product TPPM based on reactant tetraphenylporphin II The synthetic yield is 99.7%, and the purity is 99.7%.

Embodiment 2

[0055] R in the general formula (I) tetraphenylporphin used 1 = H, R 2 = H, R 3 =Cl. The metal salt is cobalt naphthenate, the molar concentration is 0.53mol / L, and the solvent is DMF. The molar concentration of tetraphenylporphine is 0.06mol / L, and the solvent is DMF. The volume flow rate of tetraphenylporphine solution is 1.01ml / L, and the molar flow ratio of metal salt to tetraphenylporphine is 6.6:1. The reaction pressure of the reactor is 0.6MPa, the reaction temperature is 168.1°C, and the residence time is 300s. Final product TPPM based on reactant tetraphenylporphin II The synthetic yield is 99.7%, and the purity is 99.7%.

Embodiment 3

[0057] R in the general formula (I) tetraphenylporphin used 1 = H, R 2 =CH 3 , R 3 =H. The metal salt is manganese acetylacetonate, the molar concentration is 0.44mol / L, and the solvent is DMF. The molar concentration of tetraphenylporphin is 0.05 mol / L, and the solvent is a mixture of 80% by mass of DMF and 20% by mass of acetic acid. The volume flow rate of tetraphenylporphine solution is 0.87ml / L, and the molar flow ratio of metal salt to tetraphenylporphine is 5.8:1. The reaction pressure of the reactor is 0.5MPa, the reaction temperature is 161.4°C, and the residence time is 360s. Final product TPPM based on reactant tetraphenylporphin II The synthetic yield is 99.8%, and the purity is 99.6%.

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Abstract

The invention relates to a continuous preparation method of tetraphenyl divalent monometal porphyrin. The method includes the steps of dissolving tetraphenyl porphyrin and divalent metal salt in solvent respectively, and continuously adding the solution into a reactor to react, wherein the mole flow ratio of tetraphenyl porphyrin to divalent metal salt is 1:(3-10), the reaction pressure is 0.1-1.0 MPa, the reaction temperature is 135-200 DEG C, and the stay time is 10-600 s; continuously obtaining reaction solutions, and collecting the reaction solutions to be cooled, crystallized, filtered and washed to obtain the product tetraphenyl divalent monometal porphyrin. The method has the advantages of being high in yield, high in reaction efficiency, low in energy consumption, safe and environmentally friendly.

Description

technical field [0001] The invention relates to a continuous preparation method of tetraphenyl divalent monometal porphyrin, which belongs to the field of organic synthesis. Background technique [0002] Tetraphenyl divalent monometalloporphyrin (hereinafter referred to as TPPM II ) has the following general formula: [0003] [0004] where M stands for metal, R 1 , R 2 and R 3 Both represent substituents. [0005] TPPM II It is an intermediate of porphyrin solar cell sensitizers, and can be used to synthesize porphyrin dye sensitizers with more structures, thus providing more possibilities for its application in dye-sensitized solar cells. At the same time, metalloporphyrin compounds play an important role in medicine, biology, catalysis, materials, etc., which have aroused widespread interest and have great application potential. [0006] The above TPPM is currently synthesized II The method is mainly a liquid phase method, which is a method in which tetraphenyl...

Claims

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Application Information

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IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 王勤波熊振华
Owner 山东有言环保科技有限公司